CN102602946B - Method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate - Google Patents
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- CN102602946B CN102602946B CN201210076138.0A CN201210076138A CN102602946B CN 102602946 B CN102602946 B CN 102602946B CN 201210076138 A CN201210076138 A CN 201210076138A CN 102602946 B CN102602946 B CN 102602946B
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Abstract
The invention provides a method for preparing white carbon black with high specific surface by recycling wastewater containing sodium sulfate, the method adopts wastewater rich in sodium sulfate obtained after preparing white carbon black by a sulfuric acid precipitation method as a reaction medium, recycles the wastewater for producing the white carbon black by the sulfuric acid precipitation method, simultaneously combines optimization of production process technology, can produce white carbon black products with high specific surface, furthest utilizes sodium sulfate and water resources in the wastewater, reduces production cost, fundamentally solves the problems of environmental pollution and resource waste caused by wastewater discharge, and has remarkable social and economic benefits.
Description
Technical Field
The invention relates to a method for preparing white carbon black with a high specific surface area by recycling wastewater containing sodium sulfate.
Background
White carbon black is an amorphous silicon dioxide microporous powder material, and belongs to an important chemical product. The white carbon black has larger specific surface area, generally more than 130 m2The emulsion has good dispersibility, adsorptivity, flame retardance and insulativity, good reinforcing and thickening effects and good dispersion, suspension and vibration liquefaction characteristics, and is widely applied to industries such as rubber, silicon rubber, plastics, coatings, catalysts, papermaking, medicines, food, electronics, chemical engineering and the like.
Sodium sulfate is also an important inorganic chemical product, and has wide application value in the production of sodium sulfide, sodium silicate, caustic soda, sodium silicate and other products, as well as the industries of nonferrous metallurgy, electroplating, papermaking, glass, cement, printing and dyeing, tanning, synthetic fiber, synthetic detergent, medicine and the like, and the market demand is very large. At present, sodium sulfate in industrial production is mainly prepared by dissolving, filtering, evaporating, drying and other processes of nitrate mud in a natural salt lake, and because the nitrate mud in the salt lake contains a large amount of calcium, magnesium, iron and chlorine plasmas, the industrial sodium sulfate product prepared by the method has high impurity content, higher production cost and very complex technical improvement, and the development of the sodium sulfate industry is restricted. With the development of socioeconomic, it is a real need for industrial development to actively develop a new way of sodium sulfate production.
Fresh water is another valuable resource for human survival and development, China is a country with serious shortage of fresh water resources, and the number of per capita fresh water resources in China is less than 2000 cubic meters in 2011, which is less than one fourth of the number of people in the world. The shortage of fresh water resources affects the basic daily life requirements of people in China, severely restricts the process and development of national industrialization, and is also a serious problem faced by countries in the world at present. The pollution of fresh water resources is prevented, and the development of a technology for saving and comprehensively utilizing the fresh water resources, particularly a new technology for industrial water, is urgent.
The preparation method of the white carbon black mainly comprises a physical method and a chemical method. The physical method is easy to introduce impurities in the production process, the grain diameter of the product is mostly more than tens of microns, the specific surface area is small, the grade of the product is not high, and the requirement of modern industrial production is difficult to meet. The chemical method is the main method for producing white carbon black at present, and mainly comprises a precipitation method and a gas phase method. The gas phase method is the mainstream production mode for producing the nano white carbon black at present, the product quality is good, the performance is stable, the purity is higher, but the equipment investment is huge, the production process is complex, the raw materials are scarce, the energy consumption of the product is high, the yield is very low, the product price is expensive, the method can only be used for a few special high-end industries, and the actual demand of various departments in industrial production on the high-quality and low-price white carbon black products can not be met. The precipitation method is the main method for producing white carbon black products at present, wherein the sulfuric acid precipitation method is also the mainstream mode for producing white carbon black by the precipitation method, and the industrial production is usually prepared by adopting a method of neutralizing and precipitating reaction of liquid sodium silicate or sodium silicate and sulfuric acid. The sulfuric acid precipitation method has the advantages of small equipment investment, simple production process, cheap and easily-obtained raw materials, high product yield and performance price, and the like, but the self-aggregation problem among primary particles in the production process of the method is serious, the particle size is not easy to control, the particle size of the product is larger compared with that of fumed silica, the specific surface of the product is smaller, the dispersion performance of the product and the reinforcing performance to rubber are poorer, in addition, a large amount of sodium sulfate wastewater is generated in the production process, and because the cost for treating the wastewater by using the existing process and technology of a production enterprise is too high, a large amount of wastewater is discharged for a long time, so that the ecological environment is seriously harmed day by day, and simultaneously, the sodium sulfate resource and the precious fresh water resource are greatly wasted. According to statistics, the worldwide production capacity of white carbon black produced by the sulfuric acid precipitation method in recent years breaks through 120 ten thousand tons, and according to the fact that about 0.4 ton of sodium sulfate can be produced as a byproduct and about 12 tons of fresh water can be consumed when one ton of precipitated white carbon black is produced in industrial production, the content of sodium sulfate resources in wastewater of the precipitated white carbon black production industry can reach 48 ten thousand tons and about 1440 thousand tons of fresh water resources can be consumed. Therefore, the sulfuric acid precipitation method is a dilemma of industry development for a long time in the aspects of promoting environmental protection, energy conservation, comprehensive utilization of resources and good development of the industry of the production process as a mainstream production method for producing white carbon black. How to prepare the white carbon black product with high specific surface by using a sulfuric acid precipitation method, and the method has the advantages of low energy consumption and low production cost, and is a problem to be solved urgently in the industry.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate.
In order to solve the technical problems, the invention provides a method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate, which comprises the following steps:
(1) adding raw materials into a reaction medium, uniformly stirring to obtain a mixed solution, keeping the temperature of the mixed solution at 60-90 ℃, wherein the raw materials are liquid sodium silicate, and the reaction medium is wastewater containing sodium sulfate;
(2) slowly adding a sulfuric acid solution serving as a precipitator into the mixed solution, carrying out precipitation reaction at the temperature of 60-90 ℃ under a stirring state, stopping the reaction when the pH value of a reaction system is 3-9, and carrying out heat preservation and aging for 1-3 hours;
(3) filtering the reactant obtained in the step (2) at least once to obtain a white carbon black filter cake and a filtrate;
(4) washing the white carbon black filter cake with deionized water, drying and crushing to obtain the white carbon black with high specific surface area;
(5) mixing washing water obtained by washing the white carbon black filter cake in the step (4) with the filtrate obtained in the step (3) to obtain waste water containing sodium sulfate, and then standing and cooling to below 40 ℃;
(6) if no sodium sulfate crystal is precipitated in the wastewater in the step (5), the sodium sulfate crystal is recycled as the reaction medium in the step (1); and (5) if sodium sulfate crystals are precipitated in the wastewater in the step (5), recycling the wastewater from which the sodium sulfate crystals are removed as the reaction medium in the step (1).
For the sake of briefly explaining the problems, the method for preparing the white carbon black with the high specific surface area by recycling the wastewater containing the sodium sulfate is hereinafter referred to as the method.
The method takes liquid sodium silicate as a raw material, sulfuric acid as a precipitator, wastewater containing sodium sulfate as a reaction medium, and sodium sulfate in the wastewater as a dispersing agent, and the hydrolysis rate of silicate and the polymerization degree of silicate molecules are regulated and controlled in the reaction process, so that the white carbon black product with high specific surface area is prepared.
Liquid sodium silicate, also called water glass, is usually melted by heating solid sodium silicate with steam at a certain temperature and pressure, and its main component is Na2O·nSiO2Thus, the chemical reaction formula of the method can be abbreviated as follows:
in the above reaction, the particle size and quality of the white carbon black product are determined by the self-polymerization process and polymerization degree of the silicic acid molecules, so that the key points for preparing the white carbon black with the high specific surface area lie in the regulation of the self-polymerization process of the silicic acid molecules and the control of the polymerization degree of the product.
The self-polymerization mechanism of the silicic acid molecules: in the process of preparing the white carbon black by the sulfuric acid precipitation method, factors influencing the hydrolysis rate of silicate and the self-polymerization behavior of silicate molecules are complex. From the analysis of the current research situation, the method is mainly related to the pH value of the reaction system, the concentration and activity of silicate ions, the reaction temperature, the reaction time, the reaction medium, the stirring action, the dispersing agent, the drying condition and other factors. The smaller the pH value of the reaction system is, the more favorable the silicate hydrolysis is, the higher the concentration and activity of silicate ions and the higher the reaction temperature are, the higher the speed of hydrolyzing the silicate ions into silicate molecules is, the higher the probability of collision between the silicate molecules is, the higher the self-polymerization speed is, the higher the polymerization degree is, the larger the particle size of the formed white carbon black particles is, and the poorer the product performance is; therefore, measures such as strengthening mechanical stirring and shearing action, adding a proper dispersing agent, adopting proper drying conditions and the like are beneficial to the dispersion of primary precipitate particles in a system, the self-polymerization probability of silicic acid molecules is reduced, the particle size of the formed white carbon black particles is greatly reduced, and the product performance is obviously improved.
The method is based on the common white carbon black technology by using a sulfuric acid precipitation method, sodium sulfate aqueous solution with proper mass concentration replaces deionized water to be used as a reaction medium, the physicochemical action between a large amount of sodium ions and sulfate ions in the sodium sulfate solution and water molecules in the solution is utilized, the hydrolysis rate of silicate ions in a reaction system is controlled, the self-polymerization probability of precipitated silicate molecules is greatly reduced, and meanwhile, the polymerization degree of the silicate molecules forming colloidal particles is obviously reduced by combining the technical conditions of controlling the pH value, the reaction temperature and time, stirring, drying and the like of the system, so that the purpose of regulating the particle size of the white carbon black is achieved, and the high-quality white carbon black product with the high specific surface area is prepared.
The white carbon black prepared by the method has low polymerization degree, small product particle size and large specific surface area, and is a new way for preparing high-quality white carbon black with high specific surface area by a sulfuric acid precipitation method.
Compared with the prior art, the method adopts the waste water rich in sodium sulfate obtained after the white carbon black is prepared by the sulfuric acid precipitation method as a reaction medium, and recycles the waste water rich in sodium sulfate for the production of the white carbon black by the sulfuric acid precipitation method, and simultaneously combines the optimization of the production process technology, so that the white carbon black product with high specific surface area can be produced, the sodium sulfate and the water resource in the waste water can be utilized to the maximum extent, the production cost is reduced, the problems of environmental pollution and resource waste caused by waste water discharge are solved fundamentally, the pollution-free discharge can be basically achieved, and the method has remarkable social and economic benefits.
In conclusion, the method can be used for preparing the white carbon black with the high specific surface area, the wastewater generated in the production process can be fully utilized, the problem of environmental pollution caused by wastewater discharge is basically eliminated, the energy consumption is reduced, and the production cost is low.
As the optimization of the method, the white carbon black filter cake is washed by deionized water for 3-5 times in the step (4).
The drying conditions of the white carbon black filter cake in the step (4) are as follows: drying for 2-4 hours at 100-150 ℃.
And (6) separating and removing precipitated sodium sulfate crystals by adopting a centrifugal method.
And (3) as a further optimization of the method, drying the sodium sulfate crystals separated in the step (6) for 1-3 hours at the temperature of 100-150 ℃ to obtain the anhydrous sodium sulfate.
The method produces the white carbon black and simultaneously produces the by-product sodium sulfate. Sodium sulfate is continuously generated in the precipitation reaction process, the concentration and the content of sodium sulfate in the wastewater can be continuously increased until saturation along with the continuous recycling of the wastewater containing sodium sulfate, the wastewater containing saturated sodium sulfate is stood and cooled, namely, crystalline sodium sulfate is separated out, and then a separation and drying method is adopted to recover a sodium sulfate byproduct.
The sodium sulfate recovered by the method also has the characteristics of low cost, low impurity content, high purity and good quality.
The main indexes of the white carbon black with high specific surface prepared by the method are compared with the main indexes of the white carbon black prepared by the common precipitation method, which are shown in the table I:
watch 1
The main indexes of the by-product sodium sulfate prepared by the method are shown in the table II:
watch two
Detailed Description
Example 1
The method for preparing the white carbon black with the high specific surface area by recycling the wastewater containing the sodium sulfate comprises the following steps:
(1) adding 360ml of liquid sodium silicate with the mass concentration of 25% into 1100ml of wastewater with the mass concentration of sodium sulfate of 8%, uniformly stirring to obtain a mixed solution, and keeping the temperature of the mixed solution at 60 ℃;
(2) slowly adding a sulfuric acid solution with the mass concentration of 20% as a precipitator into the mixed solution, carrying out precipitation reaction at the temperature of 60 ℃ under the stirring state of 160 r/min, stopping the reaction when the pH value of the reaction system is 9, and carrying out heat preservation and aging for 3 hours;
(3) filtering the reactant obtained in the step (2) to obtain a white carbon black filter cake and a filtrate;
(4) washing the white carbon black filter cake with deionized water for 4 times, drying at 100 ℃ for 4 hours, and grinding and crushing to obtain 122.3g of white carbon black product with high specific surface;
(5) mixing washing water obtained by washing the white carbon black filter cake in the step (4) with the filtrate in the step (3) to obtain waste water containing sodium sulfate, standing and cooling to 35 ℃;
(6) at this time, no sodium sulfate crystal is precipitated from the wastewater in the step (5), and the wastewater can be continuously recycled as a reaction medium for preparing the white carbon black with the high specific surface area by a sulfuric acid precipitation method.
Example 2
The method for preparing the white carbon black with the high specific surface area by recycling the wastewater containing the sodium sulfate comprises the following steps:
(1) adding 180 ml of liquid sodium silicate with the mass concentration of 20% into 500 ml of wastewater with the mass concentration of sodium sulfate of 15%, uniformly stirring to obtain a mixed solution, and keeping the temperature of the mixed solution at 80 ℃;
(2) slowly adding a sulfuric acid solution with the mass concentration of 30% as a precipitator into the mixed solution, carrying out precipitation reaction at the temperature of 80 ℃ under the stirring state of 200 r/min, stopping the reaction when the pH value of the reaction system is 6, and carrying out heat preservation and aging for 1.5 hours;
(3) filtering the reactant obtained in the step (2) to obtain a white carbon black filter cake and a filtrate;
(4) washing the white carbon black filter cake with deionized water for 3 times, drying at 120 ℃ for 3 hours, and grinding and crushing to obtain 67.3g of white carbon black product with high specific surface;
(5) mixing washing water obtained by washing the white carbon black filter cake in the step (4) with the filtrate in the step (3) to obtain waste water containing sodium sulfate, standing and cooling to 25 ℃;
(6) at this time, no sodium sulfate crystal is precipitated from the wastewater in the step (5), and the wastewater can be continuously recycled as a reaction medium for preparing the white carbon black with the high specific surface area by a sulfuric acid precipitation method.
Example 3
The method for preparing the white carbon black with the high specific surface area by recycling the wastewater containing the sodium sulfate comprises the following steps:
(1) adding 300 ml of liquid sodium silicate with the mass concentration of 20% into 700 ml of waste water with the mass concentration of sodium sulfate of 30%, uniformly stirring to obtain a mixed solution, and keeping the temperature of the mixed solution at 90 ℃;
(2) slowly adding a sulfuric acid solution with the mass concentration of 40% as a precipitator into the mixed solution, carrying out precipitation reaction at the temperature of 90 ℃ under the stirring state of 240 r/min, stopping the reaction when the pH value of the reaction system is 3, and carrying out heat preservation and aging for 1 hour;
(3) filtering the reactant obtained in the step (2) twice to obtain a white carbon black filter cake and filtrate;
(4) combining the white carbon black filter cakes obtained in the step (3), washing with deionized water for 5 times, drying at 150 ℃ for 2 hours, and grinding and crushing to obtain 130.3g of high specific surface area white carbon black product;
(5) mixing washing water obtained by washing the white carbon black filter cake in the step (4) with the filtrate in the step (3) to obtain waste water containing sodium sulfate, standing and cooling to 20 ℃;
(6) separating out sodium sulfate crystals from the wastewater in the step (5), separating out the separated sodium sulfate crystals by adopting a centrifugal method, and drying at 110 ℃ for 3 hours to obtain 55.2g of anhydrous sodium sulfate; the wastewater after separating out the precipitated sodium sulfate crystals is used as a reaction medium for preparing the white carbon black with the high specific surface area by a sulfuric acid precipitation method for continuous recycling.
What has been described above are only three embodiments of the present invention. It should be noted that variations and modifications can be made by those skilled in the art without departing from the principle of the present invention, and these should also be construed as falling within the scope of the present invention.
Claims (3)
1. The method for preparing the white carbon black with the high specific surface area by recycling the wastewater containing the sodium sulfate is characterized by comprising the following steps of:
(1) adding 360ml of liquid sodium silicate with the mass concentration of 25% into 1100ml of wastewater with the mass concentration of sodium sulfate of 8%, uniformly stirring to obtain a mixed solution, and keeping the temperature of the mixed solution at 60 ℃;
(2) slowly adding a sulfuric acid solution with the mass concentration of 20% as a precipitator into the mixed solution, carrying out precipitation reaction at the temperature of 60 ℃ under the stirring state of 160 r/min, stopping the reaction when the pH value of the reaction system is 9, and carrying out heat preservation and aging for 3 hours;
(3) filtering the reactant obtained in the step (2) to obtain a white carbon black filter cake and a filtrate;
(4) washing the white carbon black filter cake with deionized water for 4 times, drying at 100 ℃ for 4 hours, and grinding and crushing to obtain 122.3g of white carbon black product with high specific surface;
(5) mixing washing water obtained by washing the white carbon black filter cake in the step (4) with the filtrate in the step (3) to obtain waste water containing sodium sulfate, standing and cooling to 35 ℃;
(6) at this time, no sodium sulfate crystal is separated out from the wastewater in the step (5), and the wastewater is used as a reaction medium for preparing the white carbon black with the high specific surface area by a sulfuric acid precipitation method for continuous recycling.
2. The method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate according to claim 1, characterized in that: and (5) separating and removing precipitated sodium sulfate crystals by adopting a centrifugal method in the step (6).
3. The method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate according to claim 1, characterized in that: and (4) drying the sodium sulfate crystal separated in the step (6) for 1-3 hours at the temperature of 100-150 ℃ to obtain the anhydrous sodium sulfate.
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| CN103435046B (en) * | 2013-08-06 | 2015-08-05 | 龙星化工股份有限公司 | A kind of manufacture craft of high-dispersity white carbon black of snow tire |
| CN103449458A (en) * | 2013-08-21 | 2013-12-18 | 安徽确成硅化学有限公司 | Preparation method of high-dispersivity white carbon black |
| CN106277478A (en) * | 2016-08-08 | 2017-01-04 | 田晋丞 | Sulfur acid sodium waste water treatment process in precipitated silica production process |
| CN108928827A (en) * | 2018-06-22 | 2018-12-04 | 确成硅化学股份有限公司 | A method of improving white carbon black specific surface area and Kong Rong |
| CN111153412A (en) * | 2020-01-15 | 2020-05-15 | 河南省睿博环境工程技术有限公司 | White carbon black production flow based on filtering washing liquid and sodium sulfate cyclic utilization |
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| CN1065440A (en) * | 1991-04-03 | 1992-10-21 | 大连理工大学 | White carbon black prepared by solulion induced concentrated acid |
| CN1451606A (en) * | 2003-05-26 | 2003-10-29 | 四川省地质矿产勘查开发局成都综合岩矿测试中心 | Method for preparing nano mesoporous silicon dioxide from green gram rock |
| CN101274761A (en) * | 2008-05-07 | 2008-10-01 | 上虞亿得化工有限公司 | Method for preparing white carbon black with joint production of anhydrous sodium sulfate by precipitation method |
| CN101402458A (en) * | 2008-09-04 | 2009-04-08 | 南昌大学 | Method for producing nano-scale white carbon black with rice hull ash |
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| GB2169129A (en) * | 1984-12-28 | 1986-07-02 | Ppg Industries Inc | Battery separator |
| CN1065440A (en) * | 1991-04-03 | 1992-10-21 | 大连理工大学 | White carbon black prepared by solulion induced concentrated acid |
| CN1451606A (en) * | 2003-05-26 | 2003-10-29 | 四川省地质矿产勘查开发局成都综合岩矿测试中心 | Method for preparing nano mesoporous silicon dioxide from green gram rock |
| CN101274761A (en) * | 2008-05-07 | 2008-10-01 | 上虞亿得化工有限公司 | Method for preparing white carbon black with joint production of anhydrous sodium sulfate by precipitation method |
| CN101402458A (en) * | 2008-09-04 | 2009-04-08 | 南昌大学 | Method for producing nano-scale white carbon black with rice hull ash |
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